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Dimethylamine → Thiourea, N'-(3-hydroxyphenyl)-N,N-dimethyl-

HRID 1076288
ノート
印刷プレビュー

反応式

HRID 1076288 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([N:8]=[C:9]=[S:10])[CH:5]=[CH:6][CH:7]=1.[C:11]([NH:15][C:16](=[O:18])[O-:17])([CH3:14])([CH3:13])[CH3:12].CNC>CO>[OH:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]([N:15]([CH3:16])[CH3:11])=[S:10])[CH:5]=[CH:6][CH:7]=1.[C:11]([NH:15][C:16](=[O:17])[O-:18])([CH3:14])([CH3:13])[CH3:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 674DimethylamineHCID 8200263-isothiocyanatophenolHCID 21252905Tert-butylcarbamate

生成物 2

HCID 5368133Thiourea, N'-(3-hydroxyphenyl)-N,N-dimethyl-HCID 21252905Tert-butylcarbamate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
15 °C

実験手順

1-(meta-hydroxyphenyl)-3,3-dimethyl-2-thiourea, tertbutylcarbamate is prepared by charging to a suitable vessel about 25 g. (approximately 0.1 mole) meta-hydroxyphenyl isothiocyanate, tert-butylcarbamate dissolved in about 150 ml. of methanol, and adding, with stirring about 154 g. (approximately 0.12 moles) of 40 percent aqueous dimethylamine mixed with about 50 ml. of methanol in a single increment. The mass quickly solidifies as the temperature rises from about room temperature to about 60°C. The mass is cooled to about 15°C., separated from the residual liquid by filtration, washed with four 150 ml. portions of a 75 percent methanol/25 percent water solution and dried under vacuum overnight.

後処理

  1. customby charging to a suitable vessel
  2. customrises from about room temperature to about 60°C
  3. customseparated from the residual liquid by filtration
  4. washwashed with four 150 ml
  5. dry with materialportions of a 75 percent methanol/25 percent water solution and dried under vacuum overnight

出典と根拠

ORDレコード
ord-6d39d2c9fa2743f29cca32e1a8c46bdf
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03956384

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート